805 pH
pH
Semi-quantifies H2O pH using the pH meter.
Summary: This method determines the pH of water. It is most applicable to waters with a pH ranging from 4.0 to 9.0. It does not provide information on the disassociated H-ions affecting the sensing electrode. Values are reported to the nearest 0.1 pH unit. The analysis requires approximately 5 mL of sample but 10 mL is requested to allow for quality control samples.
Method 4500-H+ (pH Value) in Standard Methods for the Examination of Water and Wastewater, 20th Edition. Clesceri, L. S., Greenberg, A. E. and Eaton, A. D., eds.; American Public Health Association; Washington D.C., 1998; pp. 4-86 - 4-91.
810 Turbidity
Turbidity
Measurement of the turbidity using a nephelometer.
Summary: Turbidity in water is caused by suspended and colloidal matter and is an expression of the optical property that causes light to be scattered and absorbed rather than transmitted. This method uses a nephelometer to measure turbidity. A nephelometer is a turbidimeter with a scattered-light detector at a 90o angle to the incident beam. Possible interferences with this method include floating debris and coarse sediment which settle out rapidly. Highly colored samples can give artificially low turbidity values. The method has a detection limit of 0.1 NTU.
Clesceri, L. S., A. E. Greenberg and A. D. Eaton. 1998. Method 2130 B. (Turbidity-Nephelometric Method). Standard Methods for the Examination of Water and Wastewater, 20th Edition.
815 ESTIMATED SOLUBLE SALTS BY ELECTRICAL CONDUCTIVITY
EC
Semi-quantifies the amount of soluble salts in H2O using the conductivity meter.
Summary: This method semi-quantifies the amounts of soluble salts in the water by measurement of the electrical conductivity (ECe) of the water sample. The higher the concentration of salt in a solution, the higher will be the electrical conductance (the reciprocal of resistance). Electrical conductivity is a function of quantity and specific types of cations and anions in the water. The method has a detection limit of approximately 0.01 dS/m. The analysis requires 10 mL of sample but 25 mL is requested to allow for quality control samples.
Method 2510 (Conductivity) in Standard Methods for the Examination of Water and Wastewater 20th Edition. Clesceri, L. S., Greenberg, A. E. and Eaton, A. D., eds. American Public Health Association; Washington D.C.; 1998; pp. 2-24 - 2-47.
820 ALKALINITY, BICARBONATE AND CARBONATE
Alkalinity, HCO3, CO3
Quantification of the bicarbonate (HCO3-) and carbonate (CO32-) in H2O by titration with dilute H2SO4 acid.
Summary: This method measures bicarbonate (HCO3-), carbonate (CO32-) and alkalinity levels in water. Quantitation is by titration with 0.025 N H2SO4. The method has a routine detection limit of 0.1 meq/L but is capable of a method detection limit for alkalinity of 2 mg CaCO3/L if requested by client.
Clesceri, L. S., A. E. Greenberg and A. D. Eaton. 1998. Method 2320 (Alkalinity). Standard Methods for the Examination of Water and Wastewater, 20th Edition.
825 CHLORIDE - ELECTROMETRIC TITRATION METHOD
Solubles: Cl
Amount of chloride based on electrometric titration of H2O by chloridometer.
Summary: This method quantifies the amount of Cl in a water sample. It is based upon the electrometric titration with silver using an automatic colorimetric/amperometric chloride titrator. The method has a detection limit of 0.1 meq L-1 Cl and is generally reproducible within 5%.
Rhoades, J. D. 1982. Soluble salts. p. 167-179. In: A. L. Page et al. (ed.) Methods of soil analysis: Part 2: Chemical and microbiological properties. Monograph Number 9 (Second Edition). ASA, Madison, WI.
830 CHLORIDE - FLOW INJECTION ANALYZER METHOD
Solubles: Cl
Amount of chloride by flow injection analyzer.
Summary: This method quantifies the amount of Cl in a water sample. Thiocyanate ion is liberated from mercuric thiocyanate by the formation of soluble mercuric chloride. In the presence of ferric ion, free thiocyanate ion forms the highly colored ferric thiocyanate, of which the absorbance is proportional to the chloride concentration. The absorbance of the ferric thiocyanate is read at 480 nm. The method has a detection limit of 0.1 meq L-1 Cl and is generally reproducible within 5%.
Diamond, D. 1994. Determination of Chloride by Flow Injection Analysis Colorimetry. QuikChem Method 10-117-07-1-B. Lachat Instruments, Milwaukee, WI.
835 SOLUBLE ELEMENTS
Solubles: Al, B, Ca, Cu, Fe, K, Mg, Mn, Na, Si, Zn
Quantitative determination by AAS, AES and ICP-AES.
Summary: This method quantitatively determines the concentration of the listed elements in water samples by flame Atomic Absorption and Emission Spectrometry (AAS, AES) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). Approximately 100 mL per sample is requested. If sample is limited, some analyses are done simultaneously so the total sample required may be reduced. The EPA recommends that water for soluble analytes be filtered and acidified at the time of collection. Lower detection limits than those listed in the table below may be possible. Contact the lab if lower detection limits are needed or if elements not listed in the table are needed.
Element MDL (mg/L) Instrument(s) Ag 0.01 ICP Al 0.05 ICP B 0.1 ICP Ca 0.5 ICP Cd 0.005 ICP Cr 0.005 ICP Cu 0.1 ICP or AAS Fe 0.1 ICP or AAS K 0.05 AES Mg 0.5 ICP Mn 0.1 ICP or AAS Mo 0.01 ICP Na 0.1 AES Ni 0.05 ICP P 0.05 ICP Pb 0.05 ICP Si 0.1 ICP Zn 0.02 ICP or AAS
EPA Method 200.7, Trace Elements in Water Solids, and Biosolids by Inductively Coupled Plasma-Atomic Emission Spectrometry
EPA Method 258.1, Potassium (AA, Direct Aspiration)
EPA Method 273.1, Sodium (AA, Direct Aspiration)
837 COPPER IN WATER BY GRAPHITE FURNACE
By Special Request
Quantitative measurement of Copper concentration in water by Graphite Furnace.
Summary: This method quantitatively measures the concentration of copper in water samples by Graphite Furnace Atomic Absorption Spectrometry (GFAAS). The method has a detection limit of approximately 0.1 ug/L for copper. The analysis requires approximately 2.5 mL of sample but 10 mL is requested to allow for quality control samples. Samples should be refrigerated and acidified until delivery to the lab.
Cabon, J.Y. and Le Bihan, A. 1995. The determination of Cr, Cu and Mn in seawater with transversely heated graphite furnace atomic absorption spectrometry. Spectrochimica Acta Part B 50 (1195) 1703-1716.
Perkin Elmer, The THGA Graphite Furnace Techniques and Recommended Conditions Manual.
840 SODIUM ADSORPTION RATIO (SAR) AND EXCHANGEABLE SODIUM PERCENTAGE (ESP)
SAR, ESP
Sodium Adsorption Ratio is an estimated calculation from calcium, magnesium and sodium in water. Exchangeable Sodium Percentage calculated from SAR values.
Summary: It is possible to estimate the sodium adsorption ratio (SAR) and exchangeable sodium percentage (ESP) after determining Ca, Mg and Na concentrations in water (SOP# 835). The method has a detection limit of 0.1 for SAR and 1% for ESP.
U.S. Salinity Laboratory Staff. 1954. Choice of determinations and interpretation of data. pp. 25-26. In: L. A. Richards (ed.) Diagnosis and improvement of saline and alkali soils. USDA Agricultural Handbook 60. U.S. Government Printing Office, Washington, D.C.
845 NITRATE AND AMMONIUM - DIFFUSION-CONDUCTIVITY ANALYZER METHOD
NO3-N, NH4-N
Determination by diffusion-conductivity analyzer.
Summary: This method involves the quantitative analysis of ammonium (NH4-N) and nitrate (NO3-N) in water. Ammonium and nitrate are measured by the diffusion-conductivity method based on the gaseous diffusing of ammonia (NH3) across a gas permeable membrane in the presence of excess base (KOH) and subsequent conductivity detection. Samples can be stored for up to three weeks at low temperature (<4°C). For longer term storage, toluene or thymol should be added to the sample to prevent microbial growth. The method has detection limit of approximately 0.05 mg L-1 and is generally reproducible within 7%.
Carlson, R. M. 1978. Automated separation and conductimetric determination of ammonia and dissolved carbon dioxide. Anal. Chem. 50:1528-1531.
847 NITRATE, NITRITE AND AMMONIUM - FLOW INJECTION ANALYZER METHOD
NO3-N, NH4-N, NO2-N
Determination by flow injection analyzer.
Summary: This method involves the quantitative analysis of ammonium (NH4-N), nitrate (NO3-N) and nitrite (NO2-N) in water. Nitrate is determined by reduction to nitrite via a copperized cadmium column. This nitrite is then determined by diazotizing with sulfanilamide followed by coupling with N-(1-naphthyl)ethlyenediaminie dihydrochloride. The absorbance of the product is measured at 520 nm. Nitrite is determined in the same manner with the cadmium column off-line. Ammonia is heated with salicylate and hypochlorite in an alkaline phosphate buffer. The presence of EDTA prevents precipitation of calcium and magnesium and sodium nitroprusside is added to enhance sensitivity. The absorbance of the reaction product is measured at 630 nm and is directly proportional to the original ammonia concentration. The method has a detection limit of approximately 0.05 mg L-1 and is generally reproducible within 7%.
Note that the nitrate values reported include any nitrite in the sample. Nitrite is typically an insignificant fraction of the nitrate.
Wendt, K. 1999. Determination of Nitrate/Nitrite by Flow Injection Analysis (Low Flow Method). QuikChem Method 10-107-04-1-A. Lachat Instruments, Milwaukee, WI.
Switala, K. 1999. Determination of Ammonia by Flow Injection analysis. QuikChem Method 10-107-06-1-A. Lachat Instruments, Milwaukee, WI.
848 AMMONIUM - DISTILLATION METHOD
By Special Request
Quantitation of Ammonium using the distillation method.
Summary: This method involves the quantitation of ammonium (NH4-N) in water and waste water. Samples are pH adjusted to pH >9.5, steam distilled into dilute sulfuric acid and analyzed by flow injection analysis (FIA). Ammonium concentration is determined by FIA using the color reaction of NH4 with salicylate, nitroprusside and hypochlorite in an alkaline phosphate buffer. The absorbance of the reaction product is measured at 660 nm. The method has a detection limit of approximately 0.5 mg/L and is generally reproducible within 8%.
The Lab requests a sample size of at least 250 mL. Samples should be frozen or refrigerated until delivered to the lab. Acidification with sulfuric acid to pH < 2 can be used as a preservative.
U.S EPA, 1999. Method 1690, Ammonia-N in Water and Biosolids by Automated Colorimetry with Preliminary Distillation.
Switala, K. 1999. Determination of Ammonia by Flow Injection analysis. QuikChem Method 10-107-06-1-A. Lachat Instruments, Milwaukee, WI.
850 TOTAL KJELDAHL NITROGEN - TKN
TKN
Total Kjeldahl Nitrogen in H2O. Total reduced nitrogen by the wet oxidation of H2O using micro Kjeldahl procedure with sulfuric acid and digestion catalyst.
Summary: The Total Kjeldahl Nitrogen (TKN) method is based on the wet oxidation of nitrogen using sulfuric acid and digestion catalyst. The procedure converts organic nitrogen to the ammonium form and subsequent determination of ammonium. The procedure does not quantitatively digest nitrogen from heterocyclic forms (bound in a carbon ring), from oxidized forms such as nitrate and nitrite. The method has a detection limit of approximately 0.1mg L-1 N and is generally reproducible within 8%.
Carlson, R. M. 1978. Automated separation and conductimetric determination of ammonia and dissolved carbon dioxide. Anal. Chem. 50:1528-1531.
860 SULFATE - SULFUR IN WATER
SO4S
Amount of sulfate-sulfur present in H2O by ICP-AES.
Summary: method quantitatively measures the concentration of soluble sulfur in the water sample. The result is based on the determination of soluble sulfur using an Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES) and assumes that all sulfur present is in the sulfate form. The ICP-AES method has a detection limit of 0.1 mg/L. The analysis requires approximately 5 mL of sample but 15 mL is requested to allow for quality control samples. If sulfate is of specific interest, the ion chromatographic method should be requested.
865 SOLUBLE PHOSPHOROUS IN WATER
PO4-P
Quantitative determination by ascorbic acid reduction of phosphomolybdate complex and quantitative measurement by flow injection analysis.
Summary: This method quantitatively determines the amount of PO4-P in water. Orthophosphate concentration in water is determined spectrophotometrically by reacting with ammonium molybdate and antimony potassium tartrate under acidic conditions to form a complex. This complex is reduced with ascorbic acid to form a blue complex which absorbs light at 880 nm. The absorbance is proportional to the concentration of phosphorus in the sample. Samples are analyzed using an automated Flow Injection Analyzer (Lachat). The method has a detection limit of 0.05 mg/L. The analysis requires approximately 2 mL of sample but 10 mL is requested to allow for quality control samples.
Method 4500-P G (Flow Injection Analysis for Orthophosphate) in Standard Methods for the Examination of Water and Wastewater, 20th Edition. Clesceri, L. S.; Greenberg, A. E.; and Eaton, A. D.; eds. American Public Health Association; Washington DC; 1998. pp. 4-149 - 4-150.
870 TOTAL SOLIDS, TOTAL SUSPENDED SOLIDS, TOTAL DISSOLVED SOLIDS
TS, TSS, TDS
Quantitation of solids by oven drying and gravimetric analysis.
Summary: This method quantifies solids in water or wastewater samples using gravimetric analysis following oven drying. Solids refer to matter suspended or dissolved in the water or wastewater and may affect water or effluent quality in adverse ways. Waters with high dissolved solids generally are of inferior palatability and may induce unfavorable physiological reactions in transient consumers. Solids analyses are important in the control of biological and physical wastewater treatment processes and for assessing compliance with regulatory agency limitations. The method has a detection limit of approximately 4mg L-1 for TSS and 10mg L-1 for TDS and TS. The results are generally reproducible within 7%.
Clesceri, L. S., A. E. Greenberg and A. D. Eaton. 1998. Method 2540 B. (Total Solids), Method 2540 C. (Total Dissolved Solids) and Method 2540 D. (Total Suspended Solids). Standard Methods for the Examination of Water and Wastewater, 20th Edition.
875 HARDNESS
Hardness
Calculation of hardness from Ca and Mg.
Summary: It is possible to calculate the hardness of a water sample after determining Ca and Mg concentrations in water (SOP# 835). The method has a detection limit of 1 mg/L as CaCO3.
880 ANIONS BY ION CHROMATOGRAPHY
SO4, CL
Analysis of Sulfate and Chloride by Ion Chromatography.
Summary: This method quantitatively measures the concentration of sulfate and chloride in water samples by Ion Chromatography (IC). The method has detection limits of approximately 0.5 mg/L for sulfate and chloride. The analysis requires approximately 1 mL of sample but 5 mL is requested to allow for quality control samples. Samples should be refrigerated until delivery to the lab.
U.S. EPA Method 300.0, Determination of Inorganic Anions by Ion Chromatography, Revision 2.1, 1993.
885 TOTAL SILICA-HF
Si
Silica concentration by nitric acid/hydrogen peroxide/hydrofluoric acid digestion and ICP analysis.
Summary: This method quantitatively determines the concentration of utilizing a nitric acid/hydrogen peroxide/hydrofluoric acid microwave digestion and determination Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The methodology utilizes a pressure digestion/dissolution of the sample. The method has a detection of 0.1 mg L-1 and is generally reproducible within 8%.
Meyer, G. A. and Keliher, P. N. 1992. An overview of analysis by inductively coupled plasma-atomic emission spectrometry. p. 473-516. In: A. Montaser and D.W. Golightly (ed.) Inductively coupled plasmas in analytical atomic spectrometry. VCH Publishers Inc. New York, NY.
890 TOTAL ELEMENTS (INCLUDES PHOSPHORUS, SULFUR, POTASSIUM, CALCIUM, MAGNESIUM, SODIUM, BORON, ZINC, MANGANESE, IRON, COPPER AND MOLYBDENUM)
Water Totals: P, K, S, Ca, Mg, Na, B, Zn, Mn, Fe, Cu, Al, Cd, Cr, Pb, Mo, Ni
Microwave acid digestion/dissolution of sample and quantitative determination by AAS and ICP-AES.
Summary: This method quantitatively determines the concentration of P, S, Ca, Mg, K, Na, B, Zn, Mn, Fe, Cu, Mo and a variety of other elements utilizing a nitric acid/hydrogen peroxide microwave digestion and determination by atomic absorption spectrometry (AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The methodology utilizes a pressure digestion/dissolution of the sample and is incomplete relative to the total oxidation of organic carbon. K, Na, Zn, Cu, Mn, and Fe are analyzed by AAS and all others are analyzed by ICP-AES with vacuum spectrometer. The method has detection limits ranging from 0.1 mg Kg-1 to 0.01%. The method is generally reproducible within 8% for all analytes.
Note: This is the same method as SOP# 590.
Sah, R. N. and Miller, R. O. 1992. Spontaneous reaction for acid dissolution of biological tissues in closed vessels. Anal. Chem. 64:230-233.
Meyer, G. A. and Keliher, P. N. 1992. An overview of analysis by inductively coupled plasma-atomic emission spectrometry. p. 473-516. In: A. Montaser and D.W. Golightly (ed.) Inductively coupled plasmas in analytical atomic spectrometry. VCH Publishers Inc. New York, NY.
891 TOTAL COPPER IN WATER BY GRAPHITE FURNACE
By Special Request
Quantitative measurement of total copper in water samples by Graphite Furnace.
Summary: This method quantitatively measures the concentration of total copper in water samples by Graphite Furnace Atomic Absorption Spectrometry (GFAAS). The method has a detection limit of approximately 0.1 ug/L for copper. The analysis requires approximately 25 mL of sample but 100 mL is requested to allow for quality control samples. Samples should be acidified and refrigerated until delivery to the lab.
Cabon, J.Y. and Le Bihan, A. 1995. The determination of Cr, Cu and Mn in seawater with transversely heated graphite furnace atomic absorption spectrometry. Spectrochimica Acta Part B 50 (1195) 1703-1716.
U.S. EPA Method 200.7, Trace Elements in Water, Solids, and Biosolids by Inductively Coupled Plasma-Atomic Emission Spectrometry.
894 SELENIUM
Totals: Se
Total selenium using nitric/perchloric acid digestion/dissolution of sample. Quantitative determination by vapor generation by inductively coupled plasma atomic emission spectroscopy (ICP-AES).
Summary: This method is quantitative for selenium and is based on the wet oxidation of selenium bearing organic carbon and inorganic selenium compounds utilizing nitric, perchloric and sulfuric acids, reduction of selenate to selenite (IV), and determination by Vapor Generation Inductively-Coupled Plasma Emission Spectrometer (VG-ICP). The procedure is capable of measuring 1 ug L-1 of selenium in an aqueous solution. It is generally reproducible within 10%.
Tracy, M. L. and Moeller, G. 1990. Continuous flow vapor generation for inductively coupled argon plasma spectrometric analysis. Part 1: Selenium. J. Assoc. Off. Anal. Chem. 73:404-410.
896 ARSENIC
Totals: (Complete Digestion) As
Total arsenic, nitric/perchloric acid digestion/dissolution of sample and determination by vapor generation by inductively coupled plasma atomic emission spectroscopy (ICP-AES).
Summary: This method is quantitative for arsenic utilizing nitric, perchloric and sulfuric acids, reduction of arsenate to arsenite, and determination by Vapor Generation Inductively-Coupled Plasma Emission Spectrometer (VG-ICP). The method has a detection limit of approximately 1 ug/L. It is generally reproducible within 10%.
Tracy, M. L. and Moeller, G. 1990. Continuous flow vapor generation for inductively coupled argon plasma spectrometric analysis. Part 2: Arsenic. J. Assoc. Off. Anal. Chem. 74:516-521.
898 MERCURY
Totals: Hg
Mercury utilizing nitric acid and potassium permanganate digestion, and determination by Vapor Generation Inductively-Coupled Plasma Emission Spectrometer (VG-ICP).
Summary: This method is quantitative for mercury utilizing nitric acid and potassium permanganate digestion, and determination by Vapor Generation Inductively-Coupled Plasma Emission Spectrometer (VG-ICP). The method has a detection limit of approximately 1 ug/L. The analysis uses approximately 10 mL of sample but 50 mL is requested to allow for quality control samples.
Melton, Larry. January 26, 2000. Mercury Quantitation by Hydride Generation ICP. CAHFS Toxicology Laboratory Standard Operating Procedure. HGVICP ver 04.